spice d-limonene solubility

[burnt]

Hey someone i know sort of was doing some hypothetical work and thought you guys might find it interesting so I will repeat it here.


10mgs white spice dissolve in 1mL d-limonene easily. scale this up that means 10mL of d-limonene should dissolve 100mgs spice and 100mL d-limonene would easily dissovle 1 gram. more then 10mgs would have probaly dissolve in 1 mL but it was just a test. the 10mgs would not crystallize out of solution upon freezing. drying off the d-limonene can easily be done under light heat with a flow of air, however what is left is a yellowish liquid (mixture of d-limonene and white spice). not something easy to work with.

 

[endlessness]

thanks for the info!

as for the evapping... Is the limonene liquid remain after evapping soluble in alcohol? what about dmt freebase, is it soluble in alcohol? If any of the 2 is, then one could separate by washing with alcohol, no?


what about distiling the lemonene, would the final product be better after, and not leave the remaining oil if one would evap it afterwards?

 

[DrParadox]

SWIM read that DMT freebase is soluble in ethanol but has not conducted the experiment.

 

[burnt]

DMT freebase is very soluble in ethanol. however i think ok lets say you evap your d-limonene and you get this yellowish oily DMT saturated mess. you could redissolve this in ethanol and evaporate the ethanol and youd probaly be left with a cleaner product. although it still would not crystallize in the way it does with freezing in straight chain hydrocarbons.

 

[endlessness]

DMT freebase is very soluble in ethanol. however i think ok lets say you evap your d-limonene and you get this yellowish oily DMT saturated mess. you could redissolve this in ethanol and evaporate the ethanol and youd probaly be left with a cleaner product. although it still would not crystallize in the way it does with freezing in straight chain hydrocarbons.

why not? how do you think it would be, the final product?

could one alternatively instead of evaping the alcohol, freezing it to precipitate?

 

[burnt]

well no spice will not crystallize out of alcohol because it is too soluble in it.


what i mean is i dont think you will get the nice pretty crystals one gets during recrystallization in hexane or naptha and what not. this does not mean you will not get a crystal like material upon total evaporation. its basically that your substance does not have time to form well defined crystalline structures. it does this very nicely in a solvent like hexane because your compound slowly precipitates out of solution and finds its friends and makes a pretty crystal. in a solvent thats spice is very soluble in, this type of behavior does not happen because the substance is happy to just interact with the solvent until its gone.

why im suggesting too dissolve it in alcohol after evaporating most of your limonene is because when you start to evaporate the alcohol + limonene + spice mixture more of the limonene will go away in essence you are diluting it away into the air if that makes sense.

 

[endlessness]

any guess how would the alcohol interact with the dmt+limonene rest? would it form separate layers like nafta+basidified mix or would it mix? in the first case, then SWIM could just pipette the alcohol out into another container and evap... the result would be reasonably pure (even if not pretty crystals, as long as it is some sort of crystally/powdery consistence that is smokable, that is enough I guess)... in the second case, then it would be more complicated

 

[burnt]

i believe they would mix. as far as i know they are miscible solvents.

yea and you dont need pure pretty crystals you could always get them by recrystallizing with small amounts of hexane (or naptha or odorless mineral spirits). the only reason i suggested adding the alcohol and evap down again was to get rid of residual limonene because when you evaporate down the limonene it seems to form a yellowish oil substance that doesnt want to fully evaporate to leave just the spice. however if you have no problem with using one of the other solvents mentioned above id recommend those over alcohol because they are easier to evaporate.

im just trying to come up with solutions where one totally avoids the above mentioned organic solvents because it seems to be something people were interested in. hope it helps.

 

[endlessness]

yes its definitely much help and all the knowledge is very appreciated..

one thing I didnt understand though.. how would adding alcohol help get rid of limonene oil? wouldnt the alcohol evaporate and leave the limonene oil+dmt in the exact same situation, or would the fact that its diluted help it evaporate the oil some more?

any idea on percentage of limonene oil that remains, compared to the amount of limonene used? Is it a lot of remaining oil?

SWIM wondered in the last case, what could be done if this oil cant be eliminated, is to rub some camomile or another herb in the oil and smoke it, like some people do when they cant seem to get crystals and just get dmt oils... but then the question would remain how harsh the limonene oil is, how much is, if it has any side effects, etc..

 

[burnt]

one thing I didnt understand though.. how would adding alcohol help get rid of limonene oil? wouldnt the alcohol evaporate and leave the limonene oil+dmt in the exact same situation, or would the fact that its diluted help it evaporate the oil some more?

yea because its diluted itll give the limonene more time to evaporate before it gets all stuck with the spice gunk mixture.

any idea on percentage of limonene oil that remains, compared to the amount of limonene used? Is it a lot of remaining oil?

in my friends hypothetical experiment he didnt weigh it after drying but it seemed to be about have doubled the mass maybe more or less.

any idea on percentage of limonene oil that remains, compared to the amount of limonene used? Is it a lot of remaining oil?

not sure about this. id imagine it has a nice flavor but it might be too strong and irritate your throat.

 

[SyZyGyPSy]

Brother burnt, much appreciation for your contributions to this endeavor! <bows>

Swim has told me that smoking the limo residue is not an option... way too harsh, and too much of it, even if it were put on some herb. Plus it kept catching fire. Not worth repeating.

Acutally, there may be some hope of doing an alcohol separation type cleaning thing. Swim actually just thought of this a couple days ago, and it looks like endlessness has had the same idea. Previous experiments have shown that limonene is not soluble in lab-grade ethanol (it is, however, somewhat soluble in everclear, which must contain some kind of emulsifier). Swim knows from experience that ETOH and limo readily form two distinct layers. So far this is the only way Swim has successfully aquired freebase using limo, was by adding some lab-grade ETOH which promptly fell to the bottom, was separated, and evaporated to reveal a red spice goo that was quite potent, and quite easy/pleasant to smoke. The only problem with this is that, given the price of lab grade ethanol (~$40/litre), this method does not seem practical in the long run.

However, it makes sense that much less ETOH could be used if one were to evap the limo, then dissolve the goo in ETOH, which could then be placed in a sep funnel... one could then drain out the ETOH, leaving behind the oily film of limo residue that would presumably be floating on top.

Distilling the limo is something else Swim has been meaning to try... it should work, unless that non-evapping stuff is LOPs (limonene oxidations products), in which case the LOPs could still form after distillation and thus they could still interfere with your extraction.

 

[burnt]

Acutally, there may be some hope of doing an alcohol separation type cleaning thing. SWIM actually just thought of this a couple days ago, and it looks like endlessness has had the same idea. Previous experiments have shown that limonene is not soluble in lab-grade ethanol (it is, however, somewhat soluble in everclear, which must contain some kind of emulsifier). SWIM knows from experience that ETOH and limo readily form two distinct layers. So far this is the only way SWIM has successfully aquired freebase using limo, was by adding some lab-grade ETOH which promptly fell to the bottom, was separated, and evaporated to reveal a red spice goo that was quite potent, and quite easy/pleasant to smoke. The only problem with this is that, given the price of lab grade ethanol (~$40/litre), this method does not seem practical in the long run.

However, it makes sense that much less ETOH could be used if one were to evap the limo, then dissolve the goo in ETOH, which could then be placed in a sep funnel... one could then drain out the ETOH, leaving behind the oily film of limo residue that would presumably be floating on top.

it will make things easier that two layers are formed. the next question is what layer does the spice prefer to be in (it seems rather soluble in both)? also does small amounts of limonene dissolve in ethanol? however maybe if small amounts of limonene dissolve in ethanol then one could just evap away limonene to yellow residue, add 10 or so millliters ethanol (to conserve) and re evap that. sorry hypothetical friends are really busy but will get back to yall asap.


distillation is a nice way to recycle ones solvents however it requires some instrumentation.

 

[SyZyGyPSy]

Actually one can rig up a crude distillation apparatus rather easily by placing a curved lid upside down on a pot, and placing a bowl in the center of the pot, so that whatever evaps inside the pot drips down the lid to the center, where it condenses and falls into the bowl. Swim has been meaning to try this.

As for the solubility of spice in limo vs ETOH, it seems so little limo would be left after evap, that just the residue would float on top, so there'd be so little limo to hold the spice, that most of it would be in the alcohol. Maybe -tiny- amounts of spice would be in the limo, and maybe -tiny- amounts of limo would be in the ETOH and hence in the spice, but they'd be so small it would be negligible. The limo residue could be added to the next batch to recover whatever spice was left.

Swim knows from experience that pure lab-grade ETOH pulls good spice from limo. If there's a lot of limo then it will still hold some spice, but the residue left after evap shouldn't hold much...

Also any spice left in limo can be salted out and used orally...